Dyeing artificial silk.



TAT TNT ci ric.

FELIX KUNERT, F OFFENBACI-I-ON-THE-MAIN, GERMANY, ASSIGNOR TO THE Cd RPO- RATION OF CHEMISCHE FABRIK GRIESHEIM-ELEKTRON, 0F FRANKFORT-ON-THE- MAIN, GERMANY.

No Drawing.

To all whom it may concern:

Be it known that I, FELIX KUNERT, citizen of the German Empire, and resident of Offenbach-on-the-Main, in the Grand Duchy of Hesse, Germany, have invented new and useful Improvements in Dyeing Artificial Silk, of which the following is a specification.

. In a number of U. S. patents there are described dyestuffs, obtainable by combining a diazo-, tetrazoor diazo-azo compound not containing a sulfo group with an arylamid of 2:3-0Xynaphthoic acid, and processes for using these products for the production of fast shades on cotton.

Now I have invented an improvement in the art of producing ice colors on artificial silk by using the above mentioned dyestuffs, consisting in impregnating artificial silk with a solution of an arylamid of 2:3- oxynaphthoic acid and treating it with a non-sulfonated diazo compound. Under the term non-sulfonated diazo compound I include all diazo-, tetrazoor diazo-azo-compounds, not containing a sulfo group. A.

non-sulfonated diazo compound is specified because sulfonated diazo bodies produce colors which are insufiiciently fast to water. Since by this process it is not necessary to dye the goods at a high temperature, medium and dark shades. being producible at a moderate temperature, and since on the other hand the goods which have been impregnated with a solution of an arylamid of 2:3-oxynaphthoic acid can be developed with diazo compounds while wet, that is to say without being dried, the artificial ,silk' Specification of Letters Patent.

DYEING ARTIFICIAL SILK.

Patented Jan. 25, 1am.

Application filed August 5, 1914. Serial No. 855,305.

at about 30-40 C. For this purpose the viscose silk is well handled 3 or 4 times in an earthen pot and centrifugated. After the goods have completely cooled, they are introduced in a wet condition, that is to say without being dried, into the dye-bath containing the diazo compound, handled several times, then washed, soaped and brightened with acetic, formic or tartaric acid. The requisite solutions are made as follows:

Padding solution of the anilid of 2:3-oxynaphthoic acid.

Medium Dark shades. shades.

Anilid of 2:3-oxynaphthoic acid 40 gr 60 gr. Caustic soda lye, 34 Baum.. 68 cc 100 cc. Ricinoleate of soda or the sodium com- 75 gr 100 gr.

pound of Turkey red oil.

Made up to 10 liters... 10 liters.

The anilid of 2:3-oxynapththoic acid is stirred with the caustic soda lye and the ricinoleate of soda or the sodium compound of Turkey red oil, then covered with hot water, boiled and made up to the desired quantity.

Diazo soZntion.-300 grams of paranitroortho-toluidin are stirred with 600 cc. of hydrochloric acid 20 Baum and dissolved in 2000 cc. of boiling water; to the cooled solution are added 1500 grams of ice, and 156 grams of sodium nitrite, dissolved in 500 grams of water, are allowed to run in slowly in a thin stream, while stirring continuously; the whole is then made up with cold water to 10 liters.

Dye bath-25 liters of the above described diazo solution are filtered through calico and mixed with 7.5 liters of cold water, and shortly before dyeing 250 cc.

of a solution of sodium acetate (1:1), are added.

For a subsequent treatment the following solution may be made:2.5 liters of the diazo solution are mixed with 3.75 liters of cold water, and 250 ccm. of a solution of sodium acetate (151) are added. In this manner scarletred tints of Very great brightness and" excellent fastness, are obtained; on Elberfeld silk darker shades are obtained by using the same concentration 'of the baths, the darkest are the tints onTubize silk. The term Tubize silk is commonly employed in the art to designate nitrocellulose artificial silk.

.Ea'ample -HP1*oducti0n .on Elberfeld artificial silk of the dyestufi' obtained by combining cliae'otieed meta-amino-aeo-toluene with the anilid of 2:3-0wynaphth0i0 aoid.The Elberfeld silk is impregnated with a solution of the anilid of 2:3-oxynaphthoic acid as described in Example I and dyed in thesame manner in a dye-bath of the following constitution Diaeo solution-r450 grams of metaamino-azo-toluene are mixed with 600 cc. of boiling water and" 156 grams of sodium nitrite dissolved in 400 cc. of cold water are added. This paste is poured, while stirring continuously, into a mixture of 4000 grams of ice, 2000 cc. of water and 600 cc. of hydrochloric acid 20 Baum, and the whole ismade up to 10 liters.

Dye-bath.2.5 liters of the above described diazo solution are mixed .with 7.5 liters of cold water, and shortly before dyeing 300 cc. of a solution of sodium acetate (1:1 are added.

For a subsequent treatment the following f solution may be made: 2.5 liters of diazo solution are mixed with 3.75 liters of cold water, and 300 cc. of a solution of sodium acetate (1:1) are added.

r In this-manner bright dark red shades are obtained.

On viscose silk a little lighter, on Tubize silk darker,'tints are obtained by using the same concentration of the baths.

. Example lII-Pr0duction 0n Tubiee silk of the dyestufi obtained by combining cliaeotieed meta-niti-wortho-anisidin with i the meta-nit'ro-anilid of 2:3 omynaphthoio a0id'.The Tubize silk is impregnated with the following Padding solution made from the meta-nitraniliki of 2:3

A oxynaphthoic 'amd.

Light Medium Dark g fl f shades. shades. shades. Shades Mete-nitranilid of 23- 1.5a... 20gr.... 40 gr.... 60 gr.

oxy'naphthoic acid. Caustic soda lye 34 13 00.... 3500.... 67 00.... 10000.

Baum. p Ricinoleate of soda or 30gr '60 gr.... 100 gr... 150 gr.

the sodium com ound of Turkey redo Formaldehyde of 30% 3.75 gr 10'gr.... 20 gr.... 30 gr.

strength.

Made up to. 10 liters. 10 liters. 10 liters. loliters.

The goods are welLdried and dyed in a. dyebath of the following constitution: Diaeo s0luti0n.'340 grams of meta-nitroare added and at 5 C. 156 grams of sodium nitrite dissolved in 500 grams of cold water are allowed to run in slowly in a thin stream, while stirring continuously, and the whole is made up with cold water to 10 liters.

Dye-bath.

Light Medium Dark shades. shades. shades.

Diazo solution 750 00... 1250 00.. 2500 00.

(1 water 9250 00.. 8.50 00.. 7500 00. Solution of sodium acetate (1:1). 30 00.... 50 00.... 100 00.

The exhaustion of the dye-bath must be made good by adding liquor of double concentration. bright pink shades, like rhodamin, to dark red tints like Turkey red, of a very clear aspect can be obtained.

Example I VPi"0(lu0ti0n on viscose silk of the dyestufi' obtained by combining tet1'a The goods are then dyed as described in Example I, in a dyebath of the following constitution Diazo s0lati0n.'240 grams of dianisidin base are dissolved in 210 grams of hydrochloric acid 20 Baum and 2500 grams of boiling water; to the cooled solution are added 2000 grams of ice and 150 grams ofhydrochloric acid 20 Baum and then 160 grams of sodium nitritedissolved in 500 grams of water are allowed to run in slowly in a thin stream, while stirring continuously. The whole is made up'to 10 liters.

Dye-bath.

Light Medium Dark gfif shades. shades. shades. shades Diazo solution 500 00... 625 cc... 1250 00.. 2500 00. Solutionofcupricchlorid 50 00.... 75 00.... 150 00... 300 00.

40 Baum. I Solulfign of chromic acid 15 00.... 25 00.... 50 00.... 100 cc. Soldtion of aluminium 100 00... 120 00... 200 00... 250 00.

sulfate 12 B. Solution of sodium ace- 5O 00.... 00.... 125 00... 250 00.

tate (1:1).

Made up to 10 liters. 10 liters. 10 liters. 10 liters.

The exhaustion of the dye-bath must be made good by adding liquor of double concentration. After dyeing the goods are well washed, twice soaped and brightened with acid. In this manner light blue to bluish In this manner excellently.

black shades 01f. anexcellent intensity and beauty are obtained. 7

With other diazo-, tetrazo or diazo-azo compounds not containing a sulfo group A and with other arylamids of :3-9Xynaphthoic acid the process can be correspondingly conducted. Inevery case excellently uniform shades of-a very greatbrightness are obtained,

' Now what I claim and desire to secure by Letters Patent is the following:

1. In the art of producing ice colors on artificial silk the improvement consisting in impregnating the artificial silk with a solution of an arylamid of- 2:3-0xynaphthoic acid and treating it with a non-suL fonated diazo compound.

2. The art of dyeing artificial silk with a previously prepared non-sulfonated diazo compound, which comprises impregnating the artificial silk with a solution having a great aflinity for the artificial silk, namely a solution of an arylamid of .2z3-oxynaphthoic acid, and then treating the thus impregnated artificial silk with apreviously prepared non-sulfonated diazo compound, whereby the arylamid is coupled directly with the diazo compound.

That I claim the foregoing as my invention, I have signed my name in presence of two witnesses this 22nd day of July, 1914:.

FELIX KUNERT.

Witnesses:

PETER LAUTENsGHLAGER, FRITZ DE'sOR. 

